CN101863784A - Methods for preparing and extracting betaine and betaine hydrochloride - Google Patents
Methods for preparing and extracting betaine and betaine hydrochloride Download PDFInfo
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- CN101863784A CN101863784A CN201010193066A CN201010193066A CN101863784A CN 101863784 A CN101863784 A CN 101863784A CN 201010193066 A CN201010193066 A CN 201010193066A CN 201010193066 A CN201010193066 A CN 201010193066A CN 101863784 A CN101863784 A CN 101863784A
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Abstract
The invention discloses methods for preparing and extracting betaine and betaine hydrochloride. The method for preparing and extracting the betaine comprises the following steps of: performing neutralization reaction on sodium hydroxide solution and chloroacetic acid, when the solution temperature is reduced to between 20 and 60 DEG C, introducing liquid trimethylamine into a reaction kettle, stirring and performing full reaction; drying to dehydrate; and extracting high-purity betaine crystals by taking absolute methanol as an extracting agent through crystallization and the other means. The method for preparing and extracting the betaine hydrochloride comprises the following steps of: preparing a betaine hydrochloride crude product by directly adopting liquid-liquid reaction; and drying to dehydrate to obtain the pure betaine hydrochloride. Compared with the commonly adopted vacuum distillation method, iron exchange method, membrane separation method and other methods, the methods have the advantages of obviously low investment, good product quality, low unit consumption of raw materials and the like, and have good promotion value and market prospect.
Description
Technical field
The invention provides the preparation extracting method of a kind of trimethyl-glycine, beet alkali hydrochlorate, the preparing technical field that belongs to trimethyl-glycine and hydrochloride thereof is specifically related to a kind of method preparation that utilizes chemistry to combine with physical principle and extracts high-purity trimethyl-glycine, beet alkali hydrochlorate.
Background technology
The chemical name of trimethyl-glycine is a trimethylaminyl ethlyl lactone, and molecular formula is: C
5H
11NO
2, molecular weight: 117.15, be the mobile crystalline flour of white, fusing point: 293 ℃ (decomposition).Contents on dry basis requires 〉=99%, and the beet alkali hydrochlorate molecular formula is: C
5H
11NO
2HCl, molecular weight: 153.6, for white to little yellow crystalline powder, flavor is sour and astringent, soluble in water, ethanol is insoluble in ether, trichloromethane, meets alkali reaction.Fusing point 241-242 ℃, beet alkali hydrochlorate content requirement 〉=98%.
Trimethyl-glycine has the Animal lipid metabolism of promotion, relaxes effects such as stress, regulating osmotic pressure, is very important a kind of fodder additives.In recent years, along with people to the deepening continuously of trimethyl-glycine research, its many premium propertiess are found and begin to be carried out step by step utilization, high-quality BETAINE anhydrous has been widely used in medicine, field of food, market demand is increasing.
Trimethyl-glycine and hydrochloride thereof owing to limit by some specific synthesis condition, will inevitably produce a large amount of by product-sodium-chlor when being prepared by chemical synthesis process, sodium-chlor and principal product generate simultaneously, are doped in the principal product.Simultaneously, also having a small amount of heavy metal substance mixes in product.These impurity have all destroyed the quality of principal product trimethyl-glycine greatly, it must be separated fully and remove.How to accomplish the most effective separation the most completely, be the important subject of feedstuff industry always.
Find through deep market study and statistics domestic and international manufacturing enterprise, present trimethyl-glycine, beet alkali hydrochlorate production enterprise institute is the preparation extracting method of employing generally, thereby it is ubiquitous as the problems such as wherein causing the foreign matter content height of mixing of by product in the product, restricted enterprise development to a certain extent, extract 98% anhydrous type crystal type trimethyl-glycine as the domestic vacuum distilling method of generally using, the most outstanding defective of this method is, because the viscosity of mother liquor is more and more higher when distilling, though and the solubleness temperature variation of sodium-chlor in solution is also little, cause by product sodium-chlor all not separate effectively with principal product, this method is to the requirement height very of technology control, generally highly purified BETAINE anhydrous can not be obtained, the field of medicaments demand can not be satisfied.Comparatively advanced at present ion exchange method can be improved the deficiency of vacuum distillation method to a certain extent, but this method cost height, and be not suitable for large-scale industrialization production running.And the invention provides a kind of brand-new Production Flow Chart, advantage such as have with the ordinary method ratio that investment is low, superior product quality, raw material consumption amount are low, thereby have good popularization value.
Summary of the invention
The invention provides the preparation extracting method of a kind of trimethyl-glycine, beet alkali hydrochlorate; be intended to solve the problem that existing production technique is ubiquitous or investment is big or product purity is not high or starting material unit consumption amount is big; nowadays; the mode of biological extraction can not be met the need of market; improve chemical synthesis process with the better trimethyl-glycine of preparation quality, to advancing large-scale production significant.
Technical scheme of the present invention is: a kind of preparation extracting method of trimethyl-glycine may further comprise the steps:
(1) earlier by sodium hydroxide solution and Mono Chloro Acetic Acid generation neutralization reaction, when treating that solution temperature is reduced to 20-60 ℃, in reactor, feeds liquid trimethylamine, open stirring it is fully reacted;
(2) controlled temperature 100-200 ℃, dry to remove moisture content;
(3) utilize anhydrous methanol to extract high-purity trimethyl-glycine crystal by means such as crystallization treatment as extraction agent;
(4) methyl alcohol can be reclaimed and purified reusable edible by condenser.
The preferred technical solution of the present invention is: a kind of preparation extracting method of trimethyl-glycine may further comprise the steps:
(1) is that the sodium hydroxide solution of 20%-50% is squeezed into reactor with mass percentage concentration, in sodium hydroxide solution, adds Mono Chloro Acetic Acid then, open to stir it is fully reacted, and temperature is remained on 40-80 ℃; When treating that solution temperature is cooled to 20-60 ℃, in reactor, feed liquid trimethylamine, open stirring it is fully reacted, obtain the trimethyl-glycine mother liquor; Place concentration kettle to concentrate in this mother liquor, separate and remove the sodium chloride crystal (this step is separated the sodium-chlor that can remove 50-70% in the trimethyl-glycine mother liquor) of separating out, obtain the concentrated solution of trimethyl-glycine; The mol ratio of the sodium hydroxide in the described sodium hydroxide solution, Mono Chloro Acetic Acid, Trimethylamine 99 is a sodium hydroxide: Mono Chloro Acetic Acid: Trimethylamine 99=1: 1: 1;
(2) concentrated solution that will synthesize the gained trimethyl-glycine carries out drying treatment to slough the moisture content of remaining 70%-100%, and temperature is controlled at 100-200 ℃; Then with the 1-2 of the trimethyl-glycine concentrated solution quality after the dehydration doubly to wherein adding methyl alcohol, open stir and heating so that its thorough mixing, with temperature maintenance at 30 ℃-80 ℃; Bottom insolubles (sodium-chlor, impurity) is removed in centrifugation, obtains trimethyl-glycine-methanol solution;
(3) add the beet alkali hydrochlorate crystal in step (2) gained trimethyl-glycine-methanol solution, add-on is the 0.5%-5% of methanol quality, is concentrated into the 30%-80% of total liquor capacity amount then;
(4) step (3) gained solution is placed-10-15 ℃ environment crystallization, centrifugation obtains crystallisate, mother liquor is recycled, the BETAINE anhydrous crude product of the promptly only moisture and trace impurity of this crystallisate, gained BETAINE anhydrous crude product placed under 100 ℃ of-200 ℃ of environment further dehydrate, get final product high-pure anhydrous trimethyl-glycine.
Technical scheme of the present invention is: a kind of beet alkali hydrochlorate prepares extracting method: directly adopt liquid-liquid reactions to prepare the beet alkali hydrochlorate crude product, and 100 ℃-300 ℃ of controlled temperature, drying gets the pure product of beet alkali hydrochlorate to remove moisture content.
Further technical scheme of the present invention is: a kind of preparation extracting method of beet alkali hydrochlorate, may further comprise the steps: the synthetic concentrated solution of trimethyl-glycine is squeezed into reactor, feeding mass percentage concentration in concentrated solution is the hydrochloric acid of 20%-50%, open and stir so that it fully reacts, the mol ratio of trimethyl-glycine and hydrochloric acid is 1: 1; Can get white crystal by centrifugal separation resultant; The beet alkali hydrochlorate crude product of the promptly only moisture and trace impurity of this white crystal; Gained beet alkali hydrochlorate crude product placed under the 100-300 ℃ of environment further dehydrate, get final product high-purity beet alkali hydrochlorate.
The invention has the beneficial effects as follows: the invention provides that a kind of Production Flow Chart is simple, product purity 〉=98%, yield 〉=93%, be easy to promote and form chemosynthesis and the extracting method that trimethyl-glycine and hydrochloride thereof are produced in industrialization.Compare with each class methods such as the vacuum distillation method that generally adopts at present of routine, ion exchange method, membrane sepn have that tangible investment is low, superior product quality (sodium chloride content≤0.1%, heavy metal content (in Pb)≤10ppm, xln regular particles, glossy, color is pure), raw material consumption amount advantages such as low (material loss can be controlled in 5%, water consumption electricity low), this invention has excellent generalization values and market outlook.
Description of drawings
Fig. 1 is the preparation extraction process schema of trimethyl-glycine of the present invention and beet alkali hydrochlorate.
Embodiment
In conjunction with accompanying drawing 1 of the present invention, concrete implementation step is as follows:
Embodiment 1:
1, the preparation of trimethyl-glycine concentrated solution
(1) 30% sodium hydroxide solution is squeezed into reactor, in sodium hydroxide solution, add the pure product of Mono Chloro Acetic Acid then, open stirring and it is fully reacted, and temperature is remained on 30-45 ℃.
When (2) treating that solution temperature is reduced to 20-30 ℃, in reactor, feed liquid trimethylamine, open stirring it is fully reacted.
(3) aqueous solutions of betaine is placed concentration kettle be concentrated into 80% of original solution volume.
(4) after the sodium chloride crystal of separating out is removed in separation, obtain the trimethyl-glycine concentrated solution.
2, the preparation of BETAINE anhydrous and extraction
(1) this trimethyl-glycine concentrated solution is carried out drying treatment, to slough the moisture content of remaining 70-100%, temperature remains on 100-120 ℃.
(2) with the 1-3 of gained mixture amount doubly to wherein adding liquid methanol, open stir and heating so that its thorough mixing, and temperature remained on 40 ℃-60 ℃.
(3) add the beet alkali hydrochlorate crystal in this mixed solution, add-on is the 1%-2% of about quantity of methyl alcohol.
(4) concentrate this mixed solution to 60% of total liquor capacity amount.
(5) the bottom insolubles is removed in separation, obtains trimethyl-glycine-methanol solution.
(6) resulting solution is placed 0-3 ℃ of environment crystallization.
(7) separation obtains crystallisate, and this crystallisate i.e. the crude product of separating anhydrous trimethyl-glycine of a step.
(8) gained trimethyl-glycine crude product is placed under 180 ℃ of environment dehydrate, promptly get BETAINE anhydrous, product purity 98.5%, yield 93.5%.
Owing to the water-soluble methyl alcohol that is insoluble to of (1) sodium-chlor, dewater by drying, sodium-chlor is all separated out from the aqueous solution: (2) trimethyl-glycine is dissolved in alcoholic solvent and sodium-chlor and heavy metal are all insoluble, can effectively utilize alcohols trimethyl-glycine is separated fully with sodium-chlor, heavy metal.Therefore, through the BETAINE anhydrous that this method makes, sodium chloride content≤0.1%, heavy metal content (in Pb)≤10ppm.Thereby this method has enlarged its use territory greatly.This method technology is easy, and production cost is low, the operational condition gentleness, and product can be widely used in fields such as feed, food, makeup, medicine, biotechnological formulation, chemical industry, has huge promotional value.
3, the preparation of beet alkali hydrochlorate and extraction
(1) concentrated solution of trimethyl-glycine is squeezed into reactor, in concentrated solution, quantitatively feed the hydrochloric acid of quality percentage composition 30%, open and stir so that it fully reacts.
(2) separate resultant get final product white crystal, promptly a step is separated the beet alkali hydrochlorate crude product to this crystallisate.
(3) gained beet alkali hydrochlorate crude product is placed under 180 ℃ of environment dehydrate, be the pure product of beet alkali hydrochlorate, product purity 98.2%, yield 93.3%.
Be equipped with beet alkali hydrochlorate with this legal system, compare with traditional method, have productive rate height, product purity height and foreign matter content is low, technology is easy, production cost is low, easy handling, advantage such as environmentally friendly, thereby this method in producing, modern livestock industry has huge promotional value.
The preparation and the extraction of embodiment 2 BETAINE anhydrous
(1) is that 40% sodium hydroxide solution is squeezed into reactor with mass percentage concentration, in sodium hydroxide solution, adds Mono Chloro Acetic Acid then, open to stir it is fully reacted, and temperature is remained on 45 ℃; When treating that solution temperature is cooled to 30 ℃, in reactor, feed liquid trimethylamine, open stirring it is fully reacted; Place concentration kettle to concentrate in the trimethyl-glycine mother liquor after reaction finishes, after the sodium chloride crystal of separating out is removed in separation, obtain the concentrated solution of trimethyl-glycine; The mol ratio of the sodium hydroxide in the described sodium hydroxide solution, Mono Chloro Acetic Acid, Trimethylamine 99 is a sodium hydroxide: Mono Chloro Acetic Acid: Trimethylamine 99=1: 1: 1.
(2) concentrated solution that will synthesize the gained trimethyl-glycine carries out drying treatment to slough remaining 99.9% moisture content, and temperature is controlled at 120 ℃; Then with the 1-2 of the trimethyl-glycine concentrated solution quality after the dehydration doubly to wherein adding methyl alcohol, open stir and heating so that its thorough mixing, with temperature maintenance at 50 ℃; Bottom insolubles (sodium-chlor, impurity) is removed in centrifugation, obtains trimethyl-glycine-methanol solution;
(3) add the beet alkali hydrochlorate crystal in step (2) gained trimethyl-glycine-methanol solution, add-on is about the 1%-2% of methanol quality, is concentrated into 60% of total liquor capacity amount then;
(4) step (3) gained solution is placed-3 ℃ of environment crystallizations, centrifugation obtains crystallisate, mother liquor is recycled, the BETAINE anhydrous crude product of the promptly only moisture and trace impurity of this crystallisate, gained BETAINE anhydrous crude product placed under 100 ℃ of-200 ℃ of environment further dehydrate, get final product high-pure anhydrous trimethyl-glycine, product purity 98.2%, yield 93.2%.
The preparation and the extraction of embodiment 3 BETAINE anhydrous
(1) is that 25% sodium hydroxide solution is squeezed into reactor with mass percentage concentration, in sodium hydroxide solution, adds Mono Chloro Acetic Acid then, open to stir it is fully reacted, and temperature is remained on 40 ℃; When treating that solution temperature is cooled to 25 ℃, in reactor, feed liquid trimethylamine, open stirring it is fully reacted; Place concentration kettle to concentrate in the trimethyl-glycine mother liquor after reaction finishes, after the sodium chloride crystal of separating out is removed in separation, obtain the concentrated solution of trimethyl-glycine; The mol ratio of the sodium hydroxide in the described sodium hydroxide solution, Mono Chloro Acetic Acid, Trimethylamine 99 is a sodium hydroxide: Mono Chloro Acetic Acid: Trimethylamine 99=1: 1: 1.
(2) concentrated solution that will synthesize the gained trimethyl-glycine carries out drying treatment to slough remaining 99.95% moisture content, and temperature is controlled at 150 ℃; Then with the 1-2 of the trimethyl-glycine concentrated solution quality after the dehydration doubly to wherein adding methyl alcohol, open stir and heating so that its thorough mixing, with temperature maintenance at 40 ℃; Bottom insolubles (sodium-chlor, impurity) is removed in centrifugation, obtains trimethyl-glycine-methanol solution;
(3) add the beet alkali hydrochlorate crystal in step (2) gained trimethyl-glycine-methanol solution, add-on is 2% of a methanol quality, is concentrated into 60% of total liquor capacity amount then;
(4) step (3) gained solution is placed 0-5 ℃ of environment crystallization, centrifugation obtains crystallisate, mother liquor is recycled, the BETAINE anhydrous crude product of the promptly only moisture and trace impurity of this crystallisate, gained BETAINE anhydrous crude product placed under 100 ℃ of-200 ℃ of environment further dehydrate, get final product high-pure anhydrous trimethyl-glycine, product purity 98.3%, yield 93.3%.
Claims (5)
1. the preparation extracting method of a trimethyl-glycine is characterized in that, may further comprise the steps:
(1) earlier by sodium hydroxide solution and Mono Chloro Acetic Acid generation neutralization reaction, when treating that solution temperature is reduced to 20-60 ℃, in reactor, feeds liquid trimethylamine, open stirring it is fully reacted;
(2) controlled temperature 100-200 ℃, dry to remove moisture content;
(3) utilize anhydrous methanol to extract high-purity trimethyl-glycine crystal by crystallization treatment as extraction agent.
2. the preparation extracting method of a kind of trimethyl-glycine as claimed in claim 1 is characterized in that, the methyl alcohol of described step (3) is reclaimed by condenser and purifies recycle.
3. the preparation extracting method of a kind of trimethyl-glycine as claimed in claim 1 or 2 is characterized in that, may further comprise the steps:
(1) is that the sodium hydroxide solution of 20%-50% is squeezed into reactor with mass percentage concentration, in sodium hydroxide solution, adds Mono Chloro Acetic Acid then, open to stir it is fully reacted, and temperature is remained on 40-80 ℃; When treating that solution temperature is cooled to 20-60 ℃, in reactor, feed liquid trimethylamine, open stirring it is fully reacted, obtain the trimethyl-glycine mother liquor; Place concentration kettle to concentrate in this mother liquor, separate and remove the sodium chloride crystal of separating out, obtain the concentrated solution of trimethyl-glycine; The mol ratio of the sodium hydroxide in the described sodium hydroxide solution, Mono Chloro Acetic Acid, Trimethylamine 99 is a sodium hydroxide: Mono Chloro Acetic Acid: Trimethylamine 99=1: 1: 1;
(2) concentrated solution that will synthesize the gained trimethyl-glycine carries out drying treatment to slough the moisture content of remaining 70%-100%, and temperature is controlled at 100-200 ℃; Then with the 1-2 of the trimethyl-glycine concentrated solution quality after the dehydration doubly to wherein adding methyl alcohol, open stir and heating so that its thorough mixing, with temperature maintenance at 30 ℃-80 ℃; The bottom insolubles is removed in centrifugation, obtains trimethyl-glycine-methanol solution;
(3) add the beet alkali hydrochlorate crystal in step (2) gained trimethyl-glycine-methanol solution, add-on is the 0.5%-5% of methanol quality, is concentrated into the 30%-80% of total liquor capacity amount then;
(4) step (3) gained solution is placed-10-15 ℃ environment crystallization, centrifugation obtains crystallisate, mother liquor is recycled, this crystallisate is the BETAINE anhydrous crude product, gained BETAINE anhydrous crude product placed under 100 ℃ of-200 ℃ of environment further dehydrate, get final product high-pure anhydrous trimethyl-glycine.
4. a beet alkali hydrochlorate prepares extracting method, it is characterized in that, directly adopts liquid-liquid reactions to prepare the beet alkali hydrochlorate crude product, 100 ℃-300 ℃ of controlled temperature, and drying gets the pure product of beet alkali hydrochlorate to remove moisture content.
5. the preparation extracting method of a kind of beet alkali hydrochlorate as claimed in claim 4, may further comprise the steps: the synthetic concentrated solution of trimethyl-glycine is squeezed into reactor, feeding mass percentage concentration in concentrated solution is the hydrochloric acid of 20%-50%, open and stir so that it fully reacts, the mol ratio of trimethyl-glycine and hydrochloric acid is 1: 1; Can get white crystal by centrifugal separation resultant, the beet alkali hydrochlorate crude product of the promptly only moisture and trace impurity of this white crystal; Gained beet alkali hydrochlorate crude product placed under the 100-300 ℃ of environment further dehydrate, get final product high-purity beet alkali hydrochlorate; The preparation method of described trimethyl-glycine concentrated solution is: with mass percentage concentration is that the sodium hydroxide solution of 20%-50% is squeezed into reactor, adds Mono Chloro Acetic Acid then in sodium hydroxide solution, opens to stir it is fully reacted, and temperature is remained on 40-80 ℃; When treating that solution temperature is cooled to 20-60 ℃, in reactor, feed liquid trimethylamine, open stirring it is fully reacted, obtain the trimethyl-glycine mother liquor; Place concentration kettle to concentrate in this mother liquor, separate and remove the sodium chloride crystal of separating out, obtain the concentrated solution of trimethyl-glycine; The mol ratio of the sodium hydroxide in the described sodium hydroxide solution, Mono Chloro Acetic Acid, Trimethylamine 99 is a sodium hydroxide: Mono Chloro Acetic Acid: Trimethylamine 99=1: 1: 1.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827012A (en) * | 2011-06-16 | 2012-12-19 | 山东奥克特化工有限公司 | Betaine production technology |
| CN103804210A (en) * | 2014-02-21 | 2014-05-21 | 山东省化工研究院 | Purification method for betaine hydrochloride |
| CN105494951A (en) * | 2015-12-02 | 2016-04-20 | 山东祥维斯生物科技股份有限公司 | Method for producing 650 betaine |
| CN108440321A (en) * | 2018-04-25 | 2018-08-24 | 山东祥维斯生物科技股份有限公司 | A method of processing beet alkali hydrochlorate sodium method production technology waste liquor |
| CN109134287A (en) * | 2018-08-27 | 2019-01-04 | 山东祥维斯生物科技股份有限公司 | The method of purification of byproduct sodium chloride in a kind of glycine betaine or beet alkali hydrochlorate production |
| CN114191841A (en) * | 2021-11-30 | 2022-03-18 | 宜兴市天石饲料有限公司 | Efficient betaine crystallization method and device |
| CN114539082A (en) * | 2022-04-01 | 2022-05-27 | 山东瑞弘生物科技股份有限公司 | Environment-friendly preparation and purification method of betaine hydrochloride |
| CN117534579A (en) * | 2023-10-12 | 2024-02-09 | 重庆中润新材料股份有限公司 | Preparation method of betaine quaternary ammonium base |
| CN117534583A (en) * | 2023-10-10 | 2024-02-09 | 重庆中润新材料股份有限公司 | Preparation method and production system of betaine hydrochloride |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827012A (en) * | 2011-06-16 | 2012-12-19 | 山东奥克特化工有限公司 | Betaine production technology |
| CN103804210A (en) * | 2014-02-21 | 2014-05-21 | 山东省化工研究院 | Purification method for betaine hydrochloride |
| CN103804210B (en) * | 2014-02-21 | 2014-11-19 | 山东省化工研究院 | Purification method for betaine hydrochloride |
| CN105494951A (en) * | 2015-12-02 | 2016-04-20 | 山东祥维斯生物科技股份有限公司 | Method for producing 650 betaine |
| CN108440321A (en) * | 2018-04-25 | 2018-08-24 | 山东祥维斯生物科技股份有限公司 | A method of processing beet alkali hydrochlorate sodium method production technology waste liquor |
| CN109134287A (en) * | 2018-08-27 | 2019-01-04 | 山东祥维斯生物科技股份有限公司 | The method of purification of byproduct sodium chloride in a kind of glycine betaine or beet alkali hydrochlorate production |
| CN109134287B (en) * | 2018-08-27 | 2021-06-15 | 山东祥维斯生物科技股份有限公司 | Purification method of byproduct sodium chloride in betaine or betaine hydrochloride production |
| CN114191841A (en) * | 2021-11-30 | 2022-03-18 | 宜兴市天石饲料有限公司 | Efficient betaine crystallization method and device |
| CN114539082A (en) * | 2022-04-01 | 2022-05-27 | 山东瑞弘生物科技股份有限公司 | Environment-friendly preparation and purification method of betaine hydrochloride |
| CN117534583A (en) * | 2023-10-10 | 2024-02-09 | 重庆中润新材料股份有限公司 | Preparation method and production system of betaine hydrochloride |
| CN117534583B (en) * | 2023-10-10 | 2024-09-06 | 重庆中润新材料股份有限公司 | Preparation method and production system of betaine hydrochloride |
| CN117534579A (en) * | 2023-10-12 | 2024-02-09 | 重庆中润新材料股份有限公司 | Preparation method of betaine quaternary ammonium base |
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